CCCCCC.C([Li:11])CCC.CC(C)([O-])C.[K+].[F:18][C:19]1[C:20]([F:28])=[C:21]([F:27])[C:22]([F:26])=[C:23]([F:25])[CH:24]=1>C(OCC)C>[F:18][C:19]1[C:24]([Li:11])=[C:23]([F:25])[C:22]([F:26])=[C:21]([F:27])[C:20]=1[F:28]Inside of a 100 ml volume glass three-neck flask equipped with a 50 ml volume glass dropping funnel, temperature resistor and septum rubber was sufficiently replaced with nitrogen. Into the flask, 15.5 g (29.8 mmol) hexane solution of 15.5 wt. % butyllithium, 3.3 g (29.8 mmol) potassium tertbutoxide and 15 ml diethyl ether were charged, of which solution was cooled to -65° C. Thereafter, 5 g (29.8 mmol) pentafluorobenzene and 15 ml diethyl ether charged into the dropping funnel were added dropwise while making the inner temperature not to exceed -55° C. After the completion of dropwise addition, the reaction mixture was kept at a temperature of -65°~-55° C. with stirring to give pentafluorophenyllithium.
Wird geladen…
